CN106432960A - Novel yttrium-calcium-zinc composite heat stabilizer and preparation method thereof - Google Patents
Novel yttrium-calcium-zinc composite heat stabilizer and preparation method thereof Download PDFInfo
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- CN106432960A CN106432960A CN201610869951.1A CN201610869951A CN106432960A CN 106432960 A CN106432960 A CN 106432960A CN 201610869951 A CN201610869951 A CN 201610869951A CN 106432960 A CN106432960 A CN 106432960A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention relates to a novel yttrium-calcium-zinc composite stabilizer and a preparation method thereof. The composite stabilizer is obtained by compounding yttrium fumaropimarate, calcium stearate, zinc stearate and pentaerythritol according to a certain ratio. The yttrium fumaropimarate is prepared by allowing fumaropimaric acid to react with yttrium acetate in an anhydrous ethanol solution to obtain an yttrium fumaropimarate crude product, and then filtering, washing and drying the yttrium fumaropimarate crude product. The composite stabilizer not only is coordinated with active chlorine on PVC and effectively prevents a dehydrochlorination reaction, but also adsorbs and neutralizes hydrogen chloride and eliminates the catalytic action on PVC degradation. The novel yttrium-calcium-zinc composite stabilizer overcomes the defects that a traditional heat stabilizer is toxic and short in thermostabilization time. It is shown by a congo red test that the heat stabilizer has good thermostabilization effect, and thermostabilization time is increased to 110 min or above, however, thermostabilization time of an ordinary rare earth stabilizer is about 30 min generally. The composite stabilizer has good application prospects in the processing field of PVC.
Description
Technical field
The invention belongs to novel plastic stabilizer field in new material auxiliary agent, it is related to a kind of Novel yttrium Ca Zn composite thermally-stabilised
Agent and its preparation and the related application in igelite.
Background technology
Polrvinyl chloride (PVC) is that big scholar without a xiucai degree produces and one of thermoplastic of using in the world, it its have low cost, corrosion resistant
The features such as erosion, high intensity, PVC advantage is a lot, but haves the shortcomings that heat stability is poor.In polyvinyl chloride resin processing, hard PVC
At 180 DEG C about, the processing of flexible PVC is also required to higher temperature to processing temperature.When temperature is increased to 130 DEG C about, PVC
Resin is degraded, and discharges HCl gas, is changed into yellow from original white simultaneously, continues intensification and can be changed into black, loses
The original physics of plastics and chemical property are so as to no longer have practical value.Solve PVC heat stability difference the most directly and
Practical method is to add heat stabilizer.Industrial at present conventional heat stabilizer mainly has lead salts, metallic soap and organotin
Deng, but product be not expensive it is simply that poisonous it is impossible to meet environmental requirement.Traditional calcium stearate, zinc stearate are well recognized as
Non-toxic heat stabilizer, but it is as heat stabilizer, and its performance is still difficult to meet PVC processed and applied performance requirement, in addition its
Also poor with the compatibility of PVC.Recent domestic mainly passes through in calcium stearate, Hard Fat to the development of non-toxic heat stabilizer
On the basis of sour zinc heat stabilizer, admixture can work in coordination with the auxiliary agent improving its thermal stability；By synthesis or preparation can increase and
The compatibility of PVC, the nontoxic calcium zinc type thermal stabilizing agent of the group such as hydroxyl, aromatic radical, alcyl in the molecule.
Application number：CN200810234061.9, the applying date：20081120, open (bulletin) number：CN101486805B, public
Open (bulletin) day：20110810, applicant：Jingjiang Xuguang Plastic Co., Ltd..Disclose a kind of PVC plastic processing calcium zinc multiple
Close the preparation method of stabilizer it is characterised in that including：(1) organic acid, calcium oxide, Zinc oxide powder are dispersed in aqueous phase,
Under phase transfer catalyst effect, reaction generates calcium of organic acid zinc complexes；(2) complex that step (1) obtains is heated, plus
Enter oils and fatss thing, stir and be kept completely separate with aqueous phase to material；(3) product obtaining after separation is placed in double roller kneading machine, heating
To 130 degree, stirring, it is gradually added into antioxidant, stabilizing additive, compression molding after organic stabilizer, get product.This reaction one
Step completes, flow process is short, do not produce the three wastes；Formulation optimization, the composite calcium zinc stabilizing agent thermal efficiency of acquisition is high, stabilization time Yao Bi city
Sell product and improve 50-100%；Product is lamellar or fine granularity, no dust pollution, and it is low just to melt temperature, wide adaptability.This heat is steady
Determine agent, its performance is still difficult to meet PVC processed and applied performance requirement, and in addition it is also poor with the compatibility of PVC.
A kind of present invention Novel yttrium Ca-Zn composite heat stabilizer, includes rich horse Korean pine perfume yttrium, due in its molecular structure
Containing three-membered ring phenanthrene skeleton and double bond, improve the compatibility of itself and PVC, thus reaching the technology mesh improving its thermal stability
Mark.
Content of the invention
It is an object of the present invention to providing a kind of asepsis environment-protecting and stability is excellent for polrvinyl chloride product processing industry
Yttrium Ca-Zn composite heat stabilizer, provide the preparation method of its primary raw material richness horse Korean pine perfume yttrium simultaneously.
The technical scheme is that：
A kind of Novel yttrium Ca-Zn composite heat stabilizer, comprises rich horse Korean pine perfume yttrium, Hard Fat in described composite thermal stabilizer
Sour calcium, zinc stearate and tetramethylolmethane, the fragrant yttrium of described rich horse Korean pine, the quality of calcium stearate, zinc stearate and tetramethylolmethane
Than respectively 30-35:15-25:15-20:20-30.
As the improvement further of scheme, the preparation method of the above rich horse Korean pine perfume yttrium is no with fumaropimaric acid
React with acetic acid yttrium in hydrous ethanol solution and richness horse Korean pine perfume yttrium crude product is obtained, then through filtering, washing, dry and be obtained.
As the improvement further of scheme, in the preparation method of the above rich horse Korean pine perfume yttrium, fumaropimaric acid and vinegar
The mol ratio of sour yttrium is 1:1-2.
As the improvement further of scheme, in the preparation method of the above rich horse Korean pine perfume yttrium, fumaropimaric acid is no
It is 25-65 DEG C with acetic acid yttrium reaction temperature in hydrous ethanol solution.
As the improvement further of scheme, in the preparation method of the above described richness horse Korean pine perfume yttrium, fumaropimaric acid
In ethanol solution with the acetic acid yttrium response time be 2-4 hour.
A kind of richness horse Korean pine perfume yttrium preparation method, with fumaropimaric acid in ethanol solution the system of reacting with acetic acid yttrium
Get Fu Ma Korean pine perfume yttrium crude product, then through filtering, washing, dry and be obtained.
As the improvement further of scheme, the above fumaropimaric acid is 1 with the mol ratio of acetic acid yttrium:1-2.
As the improvement further of scheme, the above fumaropimaric acid reacts temperature in ethanol solution with acetic acid yttrium
Spend for 25-65 DEG C.
As the improvement further of scheme, when the above fumaropimaric acid is reacted with acetic acid yttrium in ethanol solution
Between be 2-4 hour.
Advantages of the present invention：
1. the present invention, on the basis of traditional calcium zinc stabilizer, with the addition of rich horse Korean pine perfume yttrium, due to rich horse Korean pine perfume yttrium
Contain three-membered ring phenanthrene skeleton and double bond in molecular structure, improve the compatibility of itself and PVC, thus reaching its heat stability of raising
The technical goal of energy.
2. applicant has carried out a series of test, concrete grammar by congo red method to the thermal stability of heat stabilizer
With reference to GB/T2917.1-2002《Blend based on vinyl chloride homo and copolymer and product release hydrogen chloride in high temperature
Mensure congo red method with any other acid product》.Draw through test, containing rich horse Korean pine perfume yttrium, calcium stearate, stearic acid
Zinc and the composite thermal stabilizer of tetramethylolmethane, it is possible to increase PVC heat stability can be carried by it as the performance of PVC heat stabilizer
Height was by more than 110 minutes, and common rare earth thermal stabilizer-stock was at 30 minutes about.
3. Colophonium is cheap, enriches, fumaropimaric acid also has potential biological degradability and biocompatibility simultaneously
The features such as.Rich horse Korean pine perfume yttrium and yttrium Ca-Zn composite heat stabilizer technique prepared therefrom are convenient and simple, have under normal temperature and pressure
Synthetic product low production cost, reaction condition is gentle, and selectivity is high, the advantages of by-product is few.
Specific embodiment
In order to be better understood from the present invention, with reference to examples of implementation, the present invention will be further described.It should be understood that this
A little embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that saying having read the present invention
After the content awarded, those skilled in the art makes various changes or changes to the present invention, and these equivalent form of values equally fall within this
Application claims limited range.
The preparation of the rich horse Korean pine perfume yttrium of embodiment 1
It is 1 according to mol ratio:1 adds fumaropimaric acid and acetic acid yttrium in a kettle., is subsequently adding ethanol solution
Finish to dissolving, start agitating device and reflux condensate device, heat to 25 DEG C, after 2 hours response time, stop heating,
Cool to room temperature, filter, filter cake absolute ethanol washing 3 times, in drying baker, 100 DEG C of freeze-day with constant temperature 6 hours, obtain high-purity
Malaysia Korean pine perfume yttrium product 1.
The preparation of the rich horse Korean pine perfume yttrium of embodiment 2
It is 1 according to mol ratio:1.5 add fumaropimaric acid and acetic acid yttrium in a kettle., are subsequently adding dehydrated alcohol molten
Liquid finishes to dissolving, starts agitating device and reflux condensate device, heats to 40 DEG C, stops adding after 3 hours response time
Heat, cools to room temperature, filters, filter cake absolute ethanol washing 3 times, and in drying baker, 100 DEG C of freeze-day with constant temperature 6 hours, obtain height
Purity Malaysia Korean pine perfume yttrium product 2.
The preparation of the rich horse Korean pine perfume yttrium of embodiment 3
It is 1 according to mol ratio:2 add fumaropimaric acid and acetic acid yttrium in a kettle., are subsequently adding ethanol solution
Finish to dissolving, start agitating device and reflux condensate device, heat to 65 DEG C, after 4 hours response time, stop heating,
Cool to room temperature, filter, filter cake absolute ethanol washing 3 times, in drying baker, 100 DEG C of freeze-day with constant temperature 6 hours, obtain high-purity
Malaysia Korean pine perfume yttrium product 3.
The preparation of the rich horse Korean pine perfume yttrium of embodiment 4
It is 1 according to mol ratio:1.8 add fumaropimaric acid and acetic acid yttrium in a kettle., are subsequently adding dehydrated alcohol molten
Liquid finishes to dissolving, starts agitating device and reflux condensate device, heats to 50 DEG C, stops adding after 3 hours response time
Heat, cools to room temperature, filters, filter cake absolute ethanol washing 3 times, and in drying baker, 100 DEG C of freeze-day with constant temperature 6 hours, obtain height
Purity Malaysia Korean pine perfume yttrium product 4.
The preparation of embodiment 5 Novel yttrium Ca-Zn composite heat stabilizer
By the rich horse Korean pine perfume yttrium 1, calcium stearate, zinc stearate and the tetramethylolmethane that prepare in embodiment 1 according to matter
Amount ratio respectively 30:15:15:20, that is, can get Novel yttrium Ca-Zn composite heat stabilizer of the present invention.
Heat stability test：
It is 50 parts according to PVC, PVC paste resin is 50 parts, DOP is 50 parts, and 6 parts of Novel yttrium Ca-Zn composite heat stabilizer is carried out
Mechanical mixture uniformly, paints the thin layer that thickness is about 1mm on a glass, plastifies 10 minutes, be cut into 2mm × 2mm at 120 DEG C
Small pieces, then carry out Congo red test, and the result heat stability time reaches 110 minutes.
The preparation of embodiment 6 Novel yttrium Ca-Zn composite heat stabilizer
By the rich horse Korean pine perfume yttrium 2, calcium stearate, zinc stearate and the tetramethylolmethane that prepare in embodiment 2 according to matter
Amount ratio respectively 31:17:16:22, that is, can get Novel yttrium Ca-Zn composite heat stabilizer of the present invention.
Heat stability test：
It is 50 parts according to PVC, PVC paste resin is 50 parts, DOP is 50 parts, and 10 parts of Novel yttrium Ca-Zn composite heat stabilizer enters
Row mechanical mixture uniformly, paints the thin layer that thickness is about 1mm on a glass, plastifies 10 minutes at 120 DEG C, be cut into 2mm ×
2mm small pieces, then carry out Congo red test, and the result heat stability time reaches 125 minutes.
The preparation of embodiment 7 Novel yttrium Ca-Zn composite heat stabilizer
By the rich horse Korean pine perfume yttrium 3, calcium stearate, zinc stearate and the tetramethylolmethane that prepare in embodiment 3 according to matter
Amount ratio respectively 32:20:18:25, that is, can get Novel yttrium Ca-Zn composite heat stabilizer of the present invention.
Heat stability test：
It is 50 parts according to PVC, PVC paste resin is 50 parts, DOP is 50 parts, and 15 parts of Novel yttrium Ca-Zn composite heat stabilizer enters
Row mechanical mixture uniformly, paints the thin layer that thickness is about 1mm on a glass, plastifies 10 minutes at 120 DEG C, be cut into 2mm ×
2mm small pieces, then carry out Congo red test, and the result heat stability time reaches 138 minutes.
The preparation of embodiment 8 Novel yttrium Ca-Zn composite heat stabilizer
By the rich horse Korean pine perfume yttrium 4, calcium stearate, zinc stearate and the tetramethylolmethane that prepare in embodiment 4 according to matter
Amount ratio respectively 334:23:19:28, that is, can get Novel yttrium Ca-Zn composite heat stabilizer of the present invention.
Heat stability test：
It is 50 parts according to PVC, PVC paste resin is 50 parts, DOP is 50 parts, and 20 parts of Novel yttrium Ca-Zn composite heat stabilizer enters
Row mechanical mixture uniformly, paints the thin layer that thickness is about 1mm on a glass, plastifies 10 minutes at 120 DEG C, be cut into 2mm ×
2mm small pieces, then carry out Congo red test, and the result heat stability time reaches 150 minutes.
The preparation of embodiment 9 Novel yttrium Ca-Zn composite heat stabilizer
By the mixture of the rich horse Korean pine perfume yttrium 1 and 3 preparing in embodiment 4, calcium stearate, zinc stearate and season penta
Tetrol is respectively 35 according to mass ratio:25:20:30, that is, can get Novel yttrium Ca-Zn composite heat stabilizer of the present invention.
Heat stability test：
It is 50 parts according to PVC, PVC paste resin is 50 parts, DOP is 50 parts, and 18 parts of Novel yttrium Ca-Zn composite heat stabilizer enters
Row mechanical mixture uniformly, paints the thin layer that thickness is about 1mm on a glass, plastifies 10 minutes at 120 DEG C, be cut into 2mm ×
2mm small pieces, then carry out Congo red test, and the result heat stability time reaches 145 minutes.
Claims (9)
1. a kind of Novel yttrium Ca-Zn composite heat stabilizer it is characterised in that:Rich horse Korean pine is comprised in described composite thermal stabilizer
Fragrant yttrium, calcium stearate, zinc stearate and tetramethylolmethane, the fragrant yttrium of described rich horse Korean pine, calcium stearate, zinc stearate and season penta 4
The mass ratio of alcohol is respectively 30-35:15-25:15-20:20-30.
2. Novel yttrium Ca-Zn composite heat stabilizer according to claim 1 it is characterised in that:Described richness horse Korean pine perfume yttrium
Preparation method is to react with acetic acid yttrium in ethanol solution with fumaropimaric acid richness horse Korean pine perfume yttrium crude product is obtained, then passes through
Filter, washing, dry and be obtained.
3. Novel yttrium Ca-Zn composite heat stabilizer according to claim 2 it is characterised in that:Described richness horse Korean pine perfume yttrium
In preparation method, fumaropimaric acid is 1 with the mol ratio of acetic acid yttrium:1-2.
4. Novel yttrium Ca-Zn composite heat stabilizer according to claim 2 it is characterised in that:Described richness horse Korean pine perfume yttrium
In preparation method, fumaropimaric acid is 25-65 DEG C with acetic acid yttrium reaction temperature in ethanol solution.
5. the Novel yttrium Ca-Zn composite heat stabilizer according to claim 3 or 4 it is characterised in that:Described Fu Mahai
In the preparation method of Colophonium yttrium, fumaropimaric acid in ethanol solution with the acetic acid yttrium response time be 2-4 hour.
6. a kind of richness horse Korean pine perfume yttrium preparation method it is characterised in that：With fumaropimaric acid in ethanol solution with vinegar
Sour yttrium reaction is obtained richness horse Korean pine perfume yttrium crude product, then through filtering, washing, dry and be obtained.
7. according to claim 6 richness horse Korean pine perfume yttrium preparation method it is characterised in that:Described fumaropimaric acid and vinegar
The mol ratio of sour yttrium is 1:1-2.
8. according to claim 7 richness horse Korean pine perfume yttrium preparation method it is characterised in that:Described fumaropimaric acid is no
It is 25-65 DEG C with acetic acid yttrium reaction temperature in hydrous ethanol solution.
9. the rich horse Korean pine perfume yttrium according to claim 7 or 8 preparation method it is characterised in that:Described fumaropimaric acid
In ethanol solution with the acetic acid yttrium response time be 2-4 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628991A (en) * | 2009-08-19 | 2010-01-20 | 西安科技大学 | Rare earth coordination compound PVC thermal stabilizer and preparation method thereof |
| CN101717466A (en) * | 2009-11-12 | 2010-06-02 | 浙江大学 | Polyvinyl chloride processing aid and preparation method thereof |
| WO2016115257A2 (en) * | 2015-01-14 | 2016-07-21 | Lawter, Inc. | Plasticizers derived from polycyclic acids or dimer fatty acids |
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2016
- 2016-09-30 CN CN201610869951.1A patent/CN106432960B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628991A (en) * | 2009-08-19 | 2010-01-20 | 西安科技大学 | Rare earth coordination compound PVC thermal stabilizer and preparation method thereof |
| CN101717466A (en) * | 2009-11-12 | 2010-06-02 | 浙江大学 | Polyvinyl chloride processing aid and preparation method thereof |
| WO2016115257A2 (en) * | 2015-01-14 | 2016-07-21 | Lawter, Inc. | Plasticizers derived from polycyclic acids or dimer fatty acids |
Non-Patent Citations (1)
| Title |
|---|
| 徐徐等: "富马海松酸的制备及纯化", 《林产业化学与工业》 * |
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